In situ growth of ni oh 2 nanostructures on substrate for glucose measurement

HANOI UNIVERSITY OF SCIENCE AND TECHNOLOGY MASTER THESIS In situ growth of Ni(OH)2 nanostructures on substate for glucose measurement VU THI OANH Oanh.VT202682M@sis.hust.edu.vn Major of Materials Science Supersivor: Dr Chu Thi Xuan Signature of Supervisor Institute International Training Institute for Materials Science (ITIMS HANOI, 05/2022 SOCIALIST REPUBLIC OF VIETNAM Independence – Freedom - Happiness CONFIRMATION OF MASTER’S THESIS ADJUSTMENT Full name of author: Vu Thi Oanh Thesis topic: In situ growth of Ni(OH)2 nanostructures on substate for glucose measurement Major: Materials Science Student ID: 20202682M The author, the supervisor, and the Committee confirmed that the author has adjusted and implemented the thesis according to the report of the Committee on May 19th, 2022 with the following contents: The thesis has been corrected for typographical errors and printing according to the opinions of the committee’s members June 2nd 2022 Supervisor Author Dr Chu Thi Xuan Vu Thi Oanh COMMITTEE’S CHAIRMAN Assoc Prof Nguyen Van Quy THESIS TOPIC In situ growth of Ni(OH)2 nanostructures on substrate for glucose measurement Acknowledgement To complete this thesis, I would like to strongly express deep gratitude to my supervisor, Dr Chu Thi Xuan, who directly instructed me as well as helped me write this thesis I would like to sincerely thank all professors, lecturers, and employees at ITIMS for their kindness to support me during a period I have already studied and worked there I sincerely thank my groupmates in Nanosensors Laboratory and many others who supported me in doing experiments and research They are my good mentors and good friends who I am really appreciated I would like to thank “The Domestic Master/Ph.D Scholarship Programme” of Vingroup Innovation Foundation (VINIF), Vingroup Big Data Institute (VINBIGDATA), code VINIF.2020.ThS.33 for supporting my master's course I also thank the project grant number B2022-BKA-25 CTVL Finally, I want to warmly thank my family who always encourages me to follow my research career Master student (Sign and write full name) Vu Thi Oanh Abstract Glucose sensor has attracted the attention of academic and industrial researchers because of its broad applications in diabetes management, food quality control and bioprocess inspection Compared with enzymatic glucose sensors, non-enzymatic glucose sensors are more relevant because of their stable, sensitive, and low-cost process The simple and low-cost synthesis of advanced nanomaterials for non-enzymatic glucose sensor is vital in practical application Here, we introduce a facile chemical method for the synthesis of nickel(II) hydroxide nanostructures on porous nickel foam (NF) for electrochemical glucose sensor The properties of the synthesized material were characterised by field-emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, high-resolution transmission electron microscopy, selected area electron diffraction, and Raman spectroscopy The fabricated materials were applied for glucose concentration measurement in 0.1 M NaOH by cyclic voltammetry and chronoamperometry The Ni(OH)2/NF sensor is stable and has excellent sensitivity with low detection limit based on the signal-to-noise ratio of and high selectivity for glucose detection in the presence of common interfering species The Ni(OH)2/Ni electrode was successfully tested in measuring glucose concentration in real serum samples The fabricated Ni(OH)2/NF electrode can be used as a low-cost, sensitive, stable and selective platform for non-enzymatic glucose sensor TABLE OF CONTENTS INTRODUCTION CHAPTER LITERATURE REVIEWS 1.1 Overview of glucose, blood sugar, and diabetes mellitus 1.2 Glucose sensors 1.2.1 Introduction of biosensor 1.2.2 Introduction of electrochemical glucose sensor 1.3 Nickel(II) hydroxide nanostructures 1.3.1 Electrochemical behaviours of Ni(OH)2 toward glucose in alkaline… ………………………………………………………………….9 1.3.2 Structure and characteristics of Ni(OH)2 nanostructures 10 1.3.3 Methods to synthesis of Ni(OH)2 nanostructures 15 CHAPTER EXPERIMENTS AND METHODS 21 2.1 Chemical and apparatus 21 2.1.1 Chemical 21 2.1.2 Apparatus 22 2.2 Ni(OH)2 nanostructures fabrication 22 2.3 Characterization of the morphologies and composition of the synthesized materials 22 2.3.1 Scanning Electron Microsope (SEM) 22 2.3.2 Transmission Electron Microscopy (TEM) 25 2.3.3 Raman scattering 28 2.4 Electrochemical measurements 29 2.4.1 Characterization of electrochemical properties of the synthesized materials 29 2.4.2 Glucose measurements 30 CHAPTER RESULTS AND DISCUSSTION 33 3.1 Morphologies and structural characteristics of the synthesized materials33 3.1.1 FESEM images of the synthesized materials 33 3.1.2 HRTEM images of the synthesized materials 34 3.1.3 Components of the synthesized materials 34 3.2 Cyclic voltammetry measurement of the synthesized materials in alkaline medium 36 3.2.1 Influence of reaction time on the electrochemical properties of the synthesized materials 36 3.2.2 CV measurements toward glucose in alkaline medium 37 3.2.3 Influence of scan rate 39 3.2.4 The stability and reproducibility 41 3.3 Chronoamperometry measurement of the synthesized materials in alkaline medium 42 3.3.1 Optimization of the statical potential applied 42 3.3.2 Construct the calibration curve for the determination of glucose concentration 44 3.4 The effect of interferences of Ni(OH)2/NF 46 3.5 Application of the synthesized electrode for glucose measurement in real samples 47 3.6 NiO nanohives based on Ni(OH)2-precursors for glucose measurement in alkaline 47 3.6.1 Formation of NiO from Ni(OH)2-precursors 47 3.6.2 Electrochemical behaviors and glucose measurements of the synthesized NiO 49 CHAPTER 4: CONCLUSIONS 54 LIST OF PUBLICATIONS 55 PUBLICATIONS IN PROGRESS 55 REFERENCES 56 ABBREVIATIONS No Abbreviations and symbols Meaning SEM Scanning Electron Microscope FESEM Field-emission scanning electron microscopy TEM Transition Electron Microscope HRTEM High resolution transmission electron microscopy SAED Selected area electron diffraction EDS/EDX Energy-dispersive X-ray spectroscopy CV Cyclic voltammetry CA Chronoamperometry NF Nickel foam 10 LOD Limit of detection 11 HMTA Hexamethylenetetramine 12 AA L-ascorbic acid 13 DA Dopamine 14 CA Citric acid monohydrate 15 DI Deionized water 16 RE Reference electrode 17 CE Counter electrode 18 WE Working electrode LIST OF TABLES Table 1.1: Unit cell parameters for the two fundamental phases of Ni(OH)2 12 Table 1.2: X-ray diff raction parameters of β-Ni(OH)2 Diff raction angles are listed for Cu Kα (λ = 1.542 Å) and Co Kα (λ = 1.789 Å) X-ray sources 12 Table 1.3: X-ray diff raction parameters of α-Ni(OH)2 calculated using the unit cell shown in figure 1.8 Diff raction angles are listed for Cu Kα (λ = 1.542 Å) and Co Kα (λ = 1.789 Å) X-ray sources 13 Table 3.1: Comparison of the performance of the synthesized Ni(OH)2/NF and other nickel-based materials for non-enzymatic glucose sensors 45 Table 3.2: Measurement of glucose concentration of real human blood serum samples 47 Table 3.3: To compare the glucose electrochemical sensing of the fabricated sensors with other nickel-based sensors 52 LIST OF FIGURES Figure 1.1: Structural chemical formulas of glucose (D-glucose) [25] Figure 1.2: Schematic representation of a biosensor [32] Figure 1.3: Schematic drawing of the first-generation glucose sensor [47] Figure 1.4: Schematic drawing of the second-generation glucose sensor [47] Figure 1.5: Schematic representation of a third-generation biosensor [47] Figure 1.6: A general scheme of the chemical and electrochemical processes that occur at a nickel hydroxide battery electrode Figure 1.7: Mechanism of oxidation-reduction electrochemical reaction between Ni(OH)2 and glucose in alkaline medium Figure 1.8: A non-enzymatic glucose sensor based on Ni(OH)2 nanoplatelet based on GCE and ECF [55] 10 Figure 1.9: The crystal structure of β-Ni(OH)2 [57] 10 Figure 1.10: The idealized crystal structure of α-Ni(OH)2 · xH2O [57] 11 Figure 1.11: X-ray diff raction patterns of Ni(OH)2 films on Ni substrates collected using a Cu Kα X-ray source [57] 11 Figure 1.12: Raman spectra of (a) β-Ni(OH)2, (b) α-Ni(OH)2 and (c) nitrateintercalated α-Ni(OH)2 [57] 14 Figure 1.13: Six methods to prepare Ni(OH)2 [57] 16 Figure 1.14: Examples of Ni(OH)2 prepared by different methods [57] 18 Figure 2.1: Images of the commercial nickel foam 21 Figure 2.2: Experiment procedure for fabrication of materials 22 Figure 2.3: SEM procedure [61] 23 Figure 2.4: Field-emission scanning electron microscopy (FESEM) with energydispersive X-ray spectroscopy (Hitachi S-4800) 24 Figure 2.5: Classification of TEM [62] 25 Figure 2.6: Working principle of TEM [62] 26 Figure 2.7: Renishaw Invia Raman Microscope 29 Figure 2.8: Cyclic voltammogram [63] 29 Figure 2.9: a) Potential step, b) the decrease of concentration of electrochemical substance, c) relationship between current and time [63] 31 Figure 2.10: Autolab electrochemical workstation (PGSTAT302N, Netherlands) 31 Figure 2.11: Scheme for electrochemical measurement diagram 32 Figure 3.1: FESEM images of (a) the bare NF and (b-d) the Ni(OH)2/NF electrodes 33 Figure 3.2: Higher magnification of FESEM images of the Ni(OH)2/NF electrodes with different reaction time 34 Figure 3.14: (a) Low and (b) high magnification FE-SEM images of the synthesized NiO/NF electrode 3.6.2 Electrochemical behaviors and glucose measurements of the synthesized NiO Electrochemical behaviors of the materials were measured in 0.1 M NaOH at room temperature figure 3.15 illustrates the cyclic voltammograms (CVs) of the bare and NiO-modified nickel foam electrodes with a scan rate of 50 mV s-1 The CVs of the NiO/NF electrodes show higher peak current signals, which indicates that the electrochemical properties of the electrode was enhanced after deposition of NiO nanohives Additionally, with no significant shift of CVs plots of three different NiO/NF electrodes synthesized under the same conditions, the synthesized electrodes presented a good reproducibility I (mA) Ni foam NiO-10m-1 NiO-10m-2 NiO-10m-3 -2 -4 -6 -1.0 -0.5 0.0 0.5 1.0 E (V vs Ag/AgCl) 1.5 Figure 3.15: CVs plots of the NF and three NiO/NF electrodes synthesized under the same conditions 49 I (mA) mM mM mM mM mM mM -2 -4 -6 -1.0 -0.5 0.0 0.5 1.0 E (V vs Ag/AgCl) 1.5 Figure 3.16: CVs plots of NiO/NF electrode in 20 mL of 0.1 M NaOH and 0, 3, 4, 5, 6, mM glucose Glucose measurements: The synthesized electrodes were applied for glucose detection Fig presents the CVs plots of NiO/NF electrode in 20 mL of 0.1 M NaOH with 0, 3, 4, 5, 6, mM glucose It is clear that the cathodic peak currents decrease when the glucose concentration rises The mechanism of glucose electrochemical oxidation relies on the electrocatalyst based on NiO In particular, NiO was oxidised to NiO(OH) (equation 3.8), then NiO(OH) oxidises glucose to gluconicacid while NiO(OH) was reduced to NiO (equation 3.9) The following equations represent the electrocatalytic oxidation mechanism [79][80]: E.q 3.8 E.q 3.9 When glucose is added into NaOH solution, part of NiO(OH) oxidases glucose to gluconic acid The amount of NiO(OH) participate to the equation 3.8 is reduced, and the cathodic peak current is then reduced The results demonstrate that syntheisised NiO/Ni is capable to apply for catalytic activities towards glucose oxidation in glucose electrochemical sensor The electrochemical properties of the NiO material are strongly dependent on its morphology and the substates [71][81][82] For example, in study reported by Salazar et al [83], the sputtered 50 thin film NiO on screen printed electrodes showed a redox reaction at high potential (~0.55 V) with Ag pseudo-reference electrode (a) 0.3 mM 0.4 mM 0.5 mM Current (mA) 0.2 mM 0.1 mM mM 0.5 V 0.6 V 0.7 V 200 300 400 500 Time (s) 600 700 800 (b) Current (mA) y = 2.39646 + 4.42381*x R2=0.99168 0.7 V 0.6 V 0.5 V 0.0 0.2 0.4 Glucose concentration (mM) 0.6 Figure 3.17: (a) Amperometric response of NiO/NF toward glucose with a concentration range between and 0.5 mM, and (b) The plot of dependence between response current and glucose concentration at different potentials 51 He et al., [71], the hollow porous NiO modified glassy carbon was used as working electrode, where the anodic and cathodic peaks were found at about 0.48 V and 0.38 V (vs Ag/AgCl) respectively They also pointed out that the addition of glucose produces an enhancement in anodic peak current and a slight shift to higher potential, but there was almost no change in current or potential of the cathodic peak Guo et al [84] used porous honeycomb-like NiO modified NF as a working electrode for glucose sensor, and they observed the anodic and cathodic peaks at about 0.58 V and 0.28 V (vs Hg/HgO), respectively In such report, the addition of glucose produces an enhancement in anodic peak current and a slight shift to higher potential, while the cathodic peak current decreases and a slightly shifts to more positive potential It means that the anodic/cathodic peaks of Ni2+/Ni3+ can be changed depending on the substrate materials and the morphology of synthesized NiO [85] Here, our sensor showed anodic peak at +0.6 V and a cathodic peak at +0.1 V versus Ag/AgCl reference electrode in 0.1 M NaOH The difference in CVs of the NiO prepared in our study can be ascribed due to the difference in the morphology of the synthesised materials and the substrate Table 3.3: To compare the glucose electrochemical sensing of the fabricated sensors with other nickel-based sensors Materials Sensitivity (mA mM-1 cm-2) LOD (µM) Reference NiO nanopetals 0.0039 [85] Ni(OH)2/C 1.3422 0.1 [86] NiS nanoclusters@NiS nanospere 0.546 0.0083 [87] NiO nanohives 6.8 5.7 This work To further study the electrocatalytic of NiO/NF for glucose oxidation, chronoamperometry was applied to measure glucose level Three voltage values were applied, that are 0.5, 0.6, and 0.7 V As shown in Fig 5a, when the glucose rises gradually from to 0.5 mM, the response current at the applied potential of 0.7 V increases linearly While the potential is at 0.5 or 0.6 V, the response currents rise nonlinearly with the increase of glucose concentration (Fig 5b) The response current at 0.7 V depends on the glucose concentration as the below function: E.q 3.10 52 Where CG is glucose concentration (mM) The sensitivity of the sensor calculated by dividing the slope to the working electrode area of 0.65 mm2 is 6.8 mA mM1 cm-2 Based on the ratio of signal-to-noise of [3], the detection limit (LOD) of the fabricated sensor was calculated at 5.7 µM These values of the fabricated sensor are compared with some other nickel-based sensors reported before (Table 1) All results indicated that the NiO/NF electrode is a capable candidate for clinical glucose detection 53 CHAPTER 4: CONCLUSIONS After the implementation of the topic and based on the analysis results presented above, we draw some conclusions as follows:  Ni(OH)2 nanohives/NF electrode was synthesized successfully by using a facile, low-cost, and instant chemical method  Nanohives with an average cavity diameter of 300–500 nm and a nanowall thickness of approximately 15 nm were homogenously formed on the surface of NF  The Ni(OH)2/NF electrode has good electrocatalytic activity toward glucose oxidation in NaOH solution with a wide linear range from to mM (R2 = 0.999), a high sensitivity (12.55 mA mM−1 cm−2), and a detection limit of 57 µM  In addition, the sensor presented good reproducibility, high stability, and good selectivity  The fabricated electrode is a potential candidate for practical application with the values of glucose recovery from 97.83% to 116.41% in real samples measured  Successfully synthesis of NiO nanohives based on Ni(OH)2-precursors, the synthesized NiO nanohives also exhibit the good electrocatalytic activity toward glucose oxidation in NaOH solution The low cost, high sensitivity, good stability, and high selectivity of the fabricated sensor indicate that the sensor has great potential application in nonenzymatic electrochemical biosensors for blood glucose detection Besides the good results that the thesis has achieved, there are still some issues that need to be studied further Thus, the next research orientation should be:  Continue to study the influence of other synthesized conditions on the formation of different structural morphologies of Ni(OH)2, to enhance the sensitivity toward glucose  In addition, the working electrodes will be decorated with metals (such as Au, Pt, Cu,…) or combined with other metal oxides (such as CuO, NiO,…) to improve the electrochemical behaviors for glucose measurements 54 LIST OF PUBLICATIONS Vu Thi Oanh, Chu Thi Xuan, Le Manh Tu, and Nguyen Duc Hoa A Simple Chemical Procedure for Direct Synthesis of NiO on Nickel Foam Electrode Applied in Non-enzymatic Glucose Electrochemical Measurements in Lecture Notes in Networks and Systems vol 366 LNNS 100–106 (Springer Science and Business Media Deutschland GmbH, 2022) Scopus Vu Thi Oanh, Chu Thi Xuan, and Nguyen Duc Hoa A highly sensitive non-enzymatic glucose electrochemical sensor based on NiO nanohives Advances in Natural Sciences: Nanoscience and Nanotechnology 12, 045012 (2021) ISI journal Q2 PUBLICATIONS IN PROGRESS Vu Thi Oanh, Chu Thi Xuan, and Nguyen Duc Hoa Instant facile method for the in situ growth of Ni(OH)2 nanohives on nickel foam for non-enzymatic electrochemical glucose sensor (Complete manuscripts for submission – ISI journal Q1) 55 REFERENCES [1] [2] Ngoc NB, Lin ZL, Ahmed W Diabetes: What challenges lie ahead for Vietnam Annals of Global Health 2020;86:1–9 https://doi.org/10.5334/aogh.2526 Jarosz M, Socha RP, Jóźwik P, Sulka GD Amperometric glucose sensor based on the Ni(OH) /Al(OH) 4− electrode obtained from a thin Ni Al foil Applied Surface Science 2017;408:96–102 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